机械活化辅助多元醇法合成锂离子正极材料LiFePO4

doi:10.3866/PKU.WHXB201202221

物理化学学报 >> 2012, Vol. 28 >> Issue (05): 1183-1188.doi: 10.3866/PKU.WHXB201202221

机械活化辅助多元醇法合成锂离子正极材料LiFePO₄

曹雁冰^1,2, 段建国¹, 姜锋², 胡国荣¹, 彭忠东¹, 杜柯¹

1. 中南大学冶金科学与工程学院, 长沙 410083;
2. 中南大学材料科学与工程学院, 长沙 410083

收稿日期:2011-11-02 修回日期:2012-02-04 发布日期:2012-04-26
通讯作者: 曹雁冰 E-mail:cybcsu@csu.edu.cn
基金资助:
国家科技支撑计划项目(2007BAE12B01)和湖南省科技计划项目(2009GK3150)资助

Synthesis of LiFePO₄ Cathode Materials by Mechanical-Activation-Assisted Polyol Processing

CAO Yan-Bing^1,2, DUAN Jian-Guo¹, JIANG Feng², HU Guo-Rong¹, PENG Zhong-Dong¹, DU Ke¹

1. School of Metallurgical Science and Engineering, Central South University, Changsha 410083, P. R. China;
2. School of Materials Science and Engineering, Central South University, Changsha 410083, P. R. China

Received:2011-11-02 Revised:2012-02-04 Published:2012-04-26
Contact: CAO Yan-Bing E-mail:cybcsu@csu.edu.cn
Supported by:
The project was supported by the National Key Technology Research and Development Program of China (2007BAE12B01) and Technology Research and Development Program of Hunan Province, China (2009GK3150).

摘要/Abstract

摘要： 以LiH₂PO₄和还原铁粉为原料, 通过机械液相活化法获得了棒状形貌的[Fe₃(PO₄)₂·8H₂O +Li₃PO₄]前驱体, 然后在三甘醇(TEG)介质中采用多元醇工艺制备了LiFePO₄材料. 为提高其电导率, 以聚乙烯醇(PVA)为碳源, 对纯相LiFePO₄进行碳包覆改性. 通过X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、恒电流充放电和电化学阻抗谱(EIS)等测试方法对制备的材料进行了表征. 结果表明:采用机械活化辅助多元醇法可在低温下合成结晶良好的LiFePO₄, 碳包覆改性的LiFePO₄/C 材料导电性能得到改善, 电荷转移阻抗减小, 1C、2C倍率下放电容比量分别为139.8、129.5 mAh·g^-1, 具有良好的倍率性能和循环稳定性.

关键词: 正极材料, LiFePO₄, 机械活化, 多元醇法, 碳包覆

Abstract: A low-temperature approach for efficient preparation of LiFePO₄ was developed. The rod-shaped [Fe₃(PO₄)₂·8H₂O + Li₃PO₄] precursor was prepared, using a mechanochemical liquid-phase activation technique, from LiH₂PO₄ and reduction iron powder. Pure LiFePO₄ was then synthesized in boiling tetra(ethylene glycol) (TEG) by polyol processing with the as-prepared precursor. In order to improve the electrical conductivity, carbon coating of the pure LiFePO₄ was carried out, using poly(vinyl alcohol) (PVA) as the carbon source. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), galvanostatic charge-discharge test and electrochemical impedance spectroscopy (EIS). The results show that well-crystallized LiFePO₄ was successfully synthesized by polyol processing at low temperature. Carbon coating significantly improves the conductive properties of LiFePO₄ and reduces charge-transfer impedance. The obtained LiFePO₄/C composite delivers specific discharge capacities of 139.8 and 129.5 mAh·g^-1 at 1C and 2C rates, respectively, displaying good cycling performance and rate capability.

Key words: Cathode Material, LiFePO₄, Mechanical activation, Polyol processing, Carbon coating

曹雁冰, 段建国, 姜锋, 胡国荣, 彭忠东, 杜柯. 机械活化辅助多元醇法合成锂离子正极材料LiFePO₄[J]. 物理化学学报, 2012, 28(05), 1183-1188. doi: 10.3866/PKU.WHXB201202221

CAO Yan-Bing, DUAN Jian-Guo, JIANG Feng, HU Guo-Rong, PENG Zhong-Dong, DU Ke. Synthesis of LiFePO₄ Cathode Materials by Mechanical-Activation-Assisted Polyol Processing[J]. Acta Phys. -Chim. Sin. 2012, 28(05), 1183-1188. doi: 10.3866/PKU.WHXB201202221

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB201202221

https://www.whxb.pku.edu.cn/CN/Y2012/V28/I05/1183

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机械活化辅助多元醇法合成锂离子正极材料LiFePO₄

Synthesis of LiFePO₄ Cathode Materials by Mechanical-Activation-Assisted Polyol Processing

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